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UNITED STATES DEPARTMENT OF AGRICULTURE 
BULLETIN No. 466 



Contribution from the Bureau of Chemistry 
CARL L. ALSBERG, Chief 



Washington, D. C. 



PROFESSIONAL PAPER 



November 3, 1917 



MAPLE SUGAR 

COMPOSITION, METHODS OF ANALYSIS, 
EFFECT OF ENVIRONMENT 



By 

A. HUGH BRYAN, Formerly Chief, Sugar Laboratory, in 

Collaboration with M. N. STRAUGHN, C. G. CHURCH, 

A. GIVEN, S. F. SHERWOOD, Assistant Chemists 



CONTENTS 



Introduction 

Definitions 

Sampling 

Methods of Analysis 

Results of Analysis 12 

Discussion of Results 27 

Canadian Maple Sugars 35 



Page 
1 
1 
3 
3 



Page 
Effect of Environment on the Composi- 
tion of Maple Sugar 36 

Changes in Composition and Color from 

Sap Sirup to Sugar Sirup 38 

Moistu-e in Maple Sugar 39 

Maple Cream, Honey, and Wax ... 41 

Conclusions 42 




WASHINGTON 

GOVERNMENT PRINTING OFFICE 

1917 



Monograph 



D. T Of Dm 
NOV 14 1917 



: : 



\ X 5S0 
.M3l3g 



UNITED STATES DEPARTMENT OF AGRICULTURE 




BULLETIN No. 466 

Contribution from the Bureau of Chemistry 
CARL L. ALSBERG, Chief 




Washington, D. C. 



PROFESSIONAL PAPER 



November 3, 1917 



MAPLE SUGAR: COMPOSITION, METHODS OF 
ANALYSIS, EFFECT OF ENVIRONMENT. 

By A. Hugh Bryan, formerly Chief, Sugar Laboratory, in collaboration with M. N. 
Straugn, C. G. Church, A. Given, and S. F. Sherwood, Assistant Chemists. 



CONTENTS. 



Introduction 

Definitions 

Sampling 

Methods of analysis 

Results of analysis 

Discussion of results 

Canadian maple sugars 35 



Page. 
1 
1 
3 
3 
12 
27 



Effect of environment on the composition of 
maple sugar 

Changes in composition and color from sap 
sirup to sugar sirup 

Moisture in maple sugar 

Maple cream, honey, and wax 

Conclusions 



Page. 

36 

38 
39 
41 

42 



INTRODUCTION. 

A previous publication 1 of the Bureau of Chemistry dealing with 

the manufacture of maple-sap sirup gives the distinguishing features 

of sap sirup and sugar sirup, as well as the results of the chemical 

examination of 481 samples of sap sirups. The present bulletin deals 

with the methods of analysis and the composition of maple sugars 

examined in the former Sugar Laboratory of the Bureau of Chemistry 

in connection with the previous report and of samples collected during 

the seasons 1910, 1911, and 1912. It is believed that this report may 

be useful to food chemists who are called upon to examine maple 

products. 

DEFINITIONS. 

As maple sirup is the sap of the live maple tree concentrated to a 
standard density, with or without the addition of the usual clarifying 
agents, maple sugar is the solid product resulting from the further 
concentration of the sirup or of the sap, with or without the addition of 
clarifiers, and without the loss of any of its constituents other than 



61390°— Bull. 466—17- 



iU. S. Dept. Agr., Bur. Chem. Bui. 134. 
-1 



2 BULLETIN 466, U. S. DEPARTMENT OF AGEICULTUEE. 

the solids precipitated by the concentration. United States Depart- 
ment of Agriculture, Office of the Secretary, Food Inspection Deci- 
sion 161, January 3, 1916, states that "Maple sugar, maple concrete, 
is the solid product resulting from the evaporation of maple sap or 
maple sirup. Maple sirup is sirup made by the evaporation of maple 
sap or by the solution of maple concrete, and contains not more than 
thirty-five per cent (35%) of water and weighs not less than eleven 
(11) pounds to the gallon (231 cu. in.)." 

The maple sugar of commerce may be divided into soft or hard 
sugar or into stirred sugar (sometimes called grain sugar), cake sugar, 
and tub sugar. 

The terms hard sugar and soft sugar apply to the relative hardness 
of the product ; a sugar is said to be hard when it is difficult to break 
the cake and soft when the cake is easily broken. Hard sugar con- 
tains less moisture than soft sugar and is produced by boiling to a 
higher temperature; that is, by boiling it longer. Determinations 
of moisture in these two grades are given in tabular form on page 39. 

The terms stirred, cake, and tub sugar apply to the form in which 
the finished product is placed upon the market. 

Stirred or grain sugar, sometimes called " crumb" sugar, derives 
its name from the fact that it is concentrated to a rather high degree, 
then stirred during cooling and crystallization. The finished product 
resembles the ordinary commercial brown sugar, and as a rule is dry 
and slightly lumpy. The color varies from off white to fight brown, 
although there are some dark varieties. It is not often found on the 
open market, being made mostly for consumption in the farmer's 
home. Certain sections of the country, however, as Pennsylvania, 
produce a large quantity of their maple products in this form. 

Cake sugar, which may be either soft or hard, is so named because 
it is molded in the form of cakes varying in size from the 1 -ounce 
cakes of the fancy confectionery trade to those weighing several 
pounds. The fancy cakes as a rule dissolve readily hi the mouth, 
while the hard cakes are not easily broken by the teeth and can be 
shipped without cracking. The larger cakes are known as brick sugar. 
The color varies from off white to black. Imported maple sugar is 
usually very dark colored. The darker varieties are strong flavored 
and have more or less taste of caramel. 

Tub sugar may be classed as a soft sugar. It gains its name from 
the fact that the makers concentrate their sirup to the desired density, 
cool slightly, and then run it into tubs of from 10 to 50 pounds 
capacity, with an average of 25 pounds. These containers are gen- 
erally wooden, although tin is sometimes used for fancy trade. 
Much of the tub sugar is of a low grade and very dark. Often it is in 
a "mushy" condition and drains badly. 



MAPLE SUGAR. 3 

SAMPLING. 

In the case of grain sugar or cake sugar that is hard and dry, sam- 
pling is comparatively easy, but with tub sugar or wet cake sugar 
there is more difficulty, because the liquid portion has drained to 
some extent and may have left practically pure sucrose. Maple 
sugar is principally sucrose, or the sugar of commerce, with a mother 
liquor surrounding the crystals which gives it its particular character- 
istic qualities. Were the mother liquor removed completely from 
the crystals of sugar, one would have the ordinary sugar of com- 
merce, granulated sugar or sucrose. Maple sugar brings its high 
price not on account of the sugar it contains but because of the agree- 
able flavoring substances which are present in the mother liquor. It 
is easily argued, then, that if this mother liquor is removed in part 
the product is not maple sugar, and a person buying it would not be 
buying maple sugar. With this point of view, it is necessary in sam- 
pling a tub of maple sugar or of any soft sugar to see that the product 
is thoroughly mixed before a sample is drawn, and that the sample 
represents both the sugar and the proportionate quantity of the mother 

liquor. 

METHODS OF ANALYSIS. 

It is the general practice in the manufacture of maple sugar not to 
skim or remove the mineral matter which is separated during the 
boiling and concentration of the sirup ; many makers cake the skim- 
mings and settlings, considering that such a procedure does not injure 
the product in any way and gives it a larger volume. In the produc- 
tion of fancy cake sugar the manufacturer usually skims and removes 
all sediment carefully before the final boiling for the caking of the 
sugar. It will be readily seen that the sugar made without skim- 
ming or filtration will have a much higher ash content than that 
which has been carefully cleansed before caking. In order to place all 
sugar samples upon a comparative basis, it is necessary in the prep- 
aration of the sample for analysis to dissolve the sugar and remove 
the suspended mineral and organic matter. Samples of maple sugar, 
especially of that made from skimmings and settlings, have been 
found with an ash content as high as 3 per cent, while sugar made 
from carefully cleansed sirup sometimes contains as little as 0.77 per 
cent. If the analysis were made on the sugar itself, it would be 
possible to add nearly two-thirds white sugar and make a product 
which, according to the ash, would not be suspected of adulteration, 
but if this adulterated sugar were made into sirup and the substances 
foreign to the sugar held in suspension were removed, the ash con- 
tent would be so reduced that adulteration of two-thirds white sugar 
would be readily seen. 



4 BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 

Jones, 1 recognizing this, recommended that all maple sugar be dis- 
solved to a standard sirup of 11 pounds to the gallon, filtered, and 
the sirup analyzed, to effect a more certain determination of the 
presence or absence of adulterants. By this treatment, even with 
the highest grades of pure maple sugar, he has never obtained a sirup 
having chemical characteristics which would place it in the list of 
adulterated products. He states that "It would seem, therefore, 
that a certain minimum amount of ash can not be removed from pure 
sugar or sugar made into sirup by the ordinary methods of filtration 
and that even the slow and complete filtering which is effected by 
this method fails to remove sufficient ash from the pure goods to 
admit even a suspicion of adulteration." 

The effect of the treatment just described is readily seen in Table I, 
where the results of the eight samples of maple sugar analyzed as sugar 
and then analyzed in the sirup condition are tabulated, the individual 
determinations in all cases being calculated to the moisture-free basis. 

Table I. — Analysis of maple sugar as sugar and as sugar sirup. 





Sample No. 


Sugar. 


Sirup. 




Total 
ash. 


Insolu- 
ble ash. 


Soluble 
ash. 


Winton 

lead 
number. 


Total 
ash. 


Insolu- 
ble ash. 


Soluble 
ash. 


"Winton 

lead 
number. 


1 


Per cent. 

0.93 

.89 

1.28 

.98 

.95 

1.22 

1.35 

1.20 


Per cent. 
0.42 
.36 
.63 
.38 
.42 
.67 
.76 
.66 


Per cent. 
0.51 
.53 
.65 
.60 
.53 
.55 
.59 
.54 


2.12 
2.14 
3.28 
2.51 
2.46 
3.25 
3.38 
3.16 


Per cent. 
0.87 
.79 
.84 
.82 
.79 
.83 
.85 
.84 


Per cent. 
0.32 
.29 
.23 
.24 
.24 
.23 
.23 
.23 


Per cent. 

0.55 

.50 

.61 

.58 
.55 
.60 
.62 
.61 


2.18 


2 


2.05 


3 


2.36 


4.. 


2.40 


5 


1.93 


6 


2.29 


7 


2.35 


8. 


215 




Average 






1.10 


.54 


.56 


2.79 


.83 


.25 


.58 


2.21 



In the sugar state the total ash varied from 1.35 to 0.89 per cent, 
a variation of 0.46 per cent, with an average of 1.10 per cent, while 
after making the sugar into sirup the range was from 0.87 to 0.79 
per cent, or a variation of only 0.08 per cent, with an average of 
0.83 per cent. In the nitration process 0.27 per cent of ash had been 
removed, which corresponds practically to the loss in insoluble ash. 
The soluble ash remained practically the same, corroborated again 
by the fact that analysis of the precipitate gives only small per- 
centages of sodium or potash salts. The lead number decreased from 
an average of 2.79 to 2.21 per cent, with variations of the sugar from 
3.38 to 2.12, or 1.26 per cent, and of the sugar sirup from 2.40 to 
1.93, 0.47 per cent. Here again by analyzing the product in the 
form of a sirup the maximum and minimum results are brought closer 
together and adulteration is more easily detected. These figures agree 
with those obtained by Jones. 1 

i Vt. Agr. Exp. Sta., 17th Ann. Rpt. (1904), p. 453; 18th Ann. Rpt. (1905), p. 327. 



MAPLE SUGAR. 5 

Table II. — Comparison of sugar and sirup results (Jones). 1 



Maple sugar. 


Sirup from same 
sugar. 


Calculated to dry 
basis from ap- 
proximately 65 
per cent solids. 


Total 
ash. 


Insolu- 
ble ash. 


Total 
ash. 


Insolu- 
ble ash. 


Total 
ash. 


Insolu- 
ble ash. 


Per cent. 
0.80 
1.08 


Per cent. 
0.34 
.64 


Per cent. 
0.56 
.52 


Per cent. 
0.22 

.18 


Per cent. 
0.86 
.80 


Per cent. 
0.34 
.28 



1 Jones does not state that the figures on "Maple sugar" were calculated to a dry basis. 
"Sirup from same sugar" are on a basis of 11 pounds to the gallon. 



The figures on 



A case has never been noted in which by this treatment the sirup 
produced gives all analytical figures below the minima discussed on 
page 45 unless the maple sugar has been adulterated by the use of 
some other sugar. 

Trials were also made to determine whether making into a sugar 
a second time tended to reduce these figures. Samples of sugar 
sirups were converted into sugar and then redissolved to a sirup of 
standard density. As shown in Tables I and II, this treatment does 
not materially change the results. 

Table III. — Analysis of sugar sirups converted into sugar and redissolved to sirup. 



Sirup from first sugaring. 


Sirup from second sugaring. 


Total 
ash. 


Insolu- 
ble ash. 


Lead 
number. 


Malic 

acid 

value. 


Total 
ash. 


Insolu- 
ble ash. 


Lead 
number. 


Malic 

acid 

value. 


Per cent. 
0.78 
.87 
.83 

.77 


Per cent. 

0.23 

.24 

.27 

.24 


1.86 
2.14 
2.22 
1.86 


0.59 
.76 
.73 
.60 


Per cent. 
0.77 
.91 

.82 
.76 


Per cent. 

0.23 

.24 

.28 

.25 


1.88 
2.22 
2.25 

1.87 


0.60 

.78 
.74 
.62 



The removal of this precipitated mineral and organic matter, 
spoken of in commercial manufacture as the refining of the maple 
sugar, is simply the removal of suspended matter contained in the 
sugar sirup. As shown by Table III, this does not tend to reduce "the 
analytical figures below the minimum for pure products. 

In a later publication * Jones calls attention to the effect of con- 
centration on the percentage of the ash and also malic acid value. 
As a liquid product is concentrated, its power of holding salts in solu- 
tion becomes less; hence one expects to find less ash in a more con- 
centrated solution than in one of lower concentration. This is true 
of maple, as shown in Table IV. 

i Vt. Agr. Exp. Sta. Bui. 167, p. 466. 



6 BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 

Table IV. — Effect of concentration of sirup on ash and malic acid values (Jones). 





Ash. 


Malic 


Concentration. 


Total. 


Soluble. 


Insolu- 
ble. 


acid 
value. 


Average of 84 sirups having over 34 per cent water 


Per cent. 

1.02 

.80 

.77 


Per cent. 

0.45 

.48 

.49 


Per cent. 

0.57 

.32 

.28 


1.00 


Average of 42 sirups having from 30 to 34 per cent water 

Average of 25 sirups having less than 30 per cent water 


.71 

.66 







i Vt. Agr. Exp. Sta. Bui. 167, p. 466. 

It is necessary, then, to use care not to concentrate a sample of sirup 
made from the sugar under examination beyond a certain point, as 
there might be a precipitation of material which would cause the 
analyst to believe the sample was adulterated. The data contained 
in Table V show the likelihood of such an occurrence. 

Table V. — Effect of addition of water on ash and malic acid values (Jones). 1 





Original sirup. 


Water added and heated. 


Sample No. 


Moist- 
ure. 


Ash. 


Malic 

acid 

value. 


Moist- 
ure. 


Ash. 


Malic 

acid 

value. 




Total. 


Solu- 
ble. 


Insolu- 
ble. 


Total. 


Solu- 
ble. 


Insolu- 
ble. 


105 


Per ct. 
30.53 
29.99 
29.46 
27.90 
29.64 
30.69 
30.94 
31.04 
26.75 
28.29 
30.70 


Per ct. 
0.79 
. 75 
.69 
.71 
.65 
.71 
.67 
.72 
.72 
. 77 
.74 


Per ct. 
0.54 
.50 
.47 
.50 
.45 
.49 
.44 
.51 
.44 
.53 
.51 


Per ct. 
0.25 
.25 
.22 
.21 
.20 
.22 
.23 
.21 
.28 
.24 
.23 


0.61 
.73 
.60 
.58 
.49 
.56 
.65 
.62 
.90 
.67 
.61 


Per ct. 
39.21 
37.25 
35.40 
35.05 
33.27 
35.75 
35.62 
38.00 
35.95 
39.40 
35.75 


Per ct. 
0.81 
.96 
.77 
.79 
.75 
.92 
.81 
.87 
.78 
.86 
.87 


Per ct. 
0.53 
.55 
.43 
.54 
.52 
.65 
.56 
.61 
.51 
.60 
.53 


P(T ct. 
0.28 
.41 
.34 
.25 
.23 
.27 
.25 
.26 
.27 
.26 
.34 


0.63 


113 




104 


.74 


107 


.61 


108 


.52 


114 


.62 


110 


.61 


115 


.60 


91 


.61 


Ill 


.66 


117 


.64 






Average 


29.63 


.72 


.49 


.23 


.64 


36.42 


.83 


.55 


.28 


.63 



i Vt. Agr. Exp. Sta. Bui. 167, p. 471. 

The original samples were concentrated in each case below the 65 
per cent solid content and showed low analytical figures in most 
cases. Taking these same samples, with the sediment contained 
therein, and adding water and boiling again to about a 35 per cent 
moisture content, the analytical figures, with the possible exception 
of No. 108, where the second concentration is below 35 per cent, are 
well within the bounds of pure products. Average figures show that 
changing the concentration from 29.63 per cent water to 36.42 per 
cent has increased the ash from 0.72 to 0.83 per cent, and the insoluble 
ash from 0.23 to 0.28 per cent, but has not changed the malic acid 
content. From this, it is seen that in concentrating the maple sugar 
sirup for analysis the dry substance of the finished sirup should not be 
much over 65 to 66 per cent. 



MAPLE SUGAR. 



COLLECTION OF SAMPLES. 



Part of the samples were collected by the authors and part by the 
official inspectors of the department from makers of maple products. 
The authenticity of these samples can not then be doubted. 

PREPARATION OF SAMPLE. 

All chemical examinations were made on a sirup prepared by disr 
solving 100 grams of the maple sugar in at least 200 cc of water, and 
boiling the solution down to a consistency of 65 per cent of solid 
matter. When an undue amount of sediment rendered the solution 
cloudy, it was boiled until the sirup consisted of about 30 per cent dry 
matter, after which it was filtered and concentrated to the 65 per cent 
basis. These solutions were kept at a temperature of 20° C. for two 
days, during which time the sediment settled, leaving a clear liquid 
for the determinations. 

The physical points ascertained were color of sugar, color of sirup, 
and taste. The chemical examination consisted in the estimation 
of sucrose, invert sugar, ash, lead number, and malic acid value, and 
qualitative test for tannin. A moisture determination was made 
on a few sugar samples. 

COLOR. 

Sugar. — The determination on sugar, at best only approximate, 
was made by comparison with the Dutch standards of color. Eight- 
een standard sugars, varying from the very dark brown grade of No. 
8 to the slightly yellowish white of No. 25, are contained in square 
glass bottles, which are filled and sealed by an association of sugar 
brokers in Amsterdam, Holland. As originally prepared, this set of 
colors was used by the Dutch to grade moist sugars coming from 
their possessions in the East India Islands, Java, etc. New sets 
identical in color with the first standards are prepared each year. 
Although grain maple sugar could be very readily compared, it was 
necessary to break up the cake or lump sugar and compare the average 
color of the broken surface with the standards. In most cases this 
color was practically that of the outside, but in some instances the 
fracture was almost white., 

Sirup. — The set of standard colors employed in the grading of 
maple-sap sirup 1 was used in this determination. 

TASTE. 

The sirups were tasted by two persons, who graded each sample 
as good, poor, or rank. 

MOISTURE IN SIRUP. 

The Abbe" heatable prism refractometer and the table of Geerlig 2 
were used for this determination. 

i U. S. Dept. Agr., Bur. Chem. Bui. 134, p. 15, pi. I. 

2 U. S. Dept. Agr., Bur. Chem. Cir. 43, p. 7; U. S. Dept. Agr., Bur. Chem. Bui. 122, p. 169; Jour. Amer. 
Chem. Soc., 30 (1909), pp. 1443-51. 



8 



BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 



SUCROSE. 

Sucrose was determined from the direct and invert polarization, 
by the Clerget formula, 1 using the factor 142.66 and hydrochloric 
acid as the hydrolyst. The results on a number of samples where 
invertase was the hydrolyst were identical with those obtained with 
the acid inversion. 

INVERT SUGAR. 

Munson and Walker's method and tables 2 were used. The pro- 
cedure, which is the same as applied to the sap sirups, is given on 
page 16 of Bureau of Chemistry Bulletin 134. 

ash. 

Five grams of the sample were ashed in a platinum dish in an elec- 
tric oven in the usual way. 3 After ashing, a few drops of ammonium 
carbonate solution were added, the whole evaporated, ignited, and 
reweighed. The same procedure was followed in the case of insoluble 
ash. Alkalinity determinations of the soluble and insoluble ash were 
also made by the usual method. 

In valuing maple products, the percentage of total ash is important 
as well as difficult to ascertain, so that the utmost care is necessary 
in carrying out this determination. Table VI shows determinations 
of ash on the same sample: (1) By burning over a free flame at a 
low heat and again at a red heat; (2) by burning in a muffle at a low 
and again at a high heat; (3) by burning in an electric oven at ordinary 
temperature. Following the results in the table are the same determi- 
nations after treatment with ammonium carbonate and reignition. 

Table VI. — Effect of method of burning on ash content. 
[Not calculated to dry basis.] 



Ex- 




peri- 


Sample 


ment 


No. 


No. 




1 


8337 


2 


9235 


3 


8337 


4 


8512 


5 


8554 



Burned. 



Temperature. 



Ash.< 



Ash after 
adding 
ammonium 
carbonate 
and heat- 
ing.* 



Free flame 

....do 

Electric muffle. 

Gas muffle 

....do 



{Free flame 
....do 
Electric muffle. 



/Free flame. 
\....do 



{' 



Free flame, 
.do 



(Free flame 
....do 
Electric muffle. 



Low . . 
High. 
, Low . . 
Low.. 
High. 

Low.. 
High.. 
Low. . 

Low . . 
High s 

Low . . 
High s 

Low . . 
High 5 
Low . . 



Per cent. 
0.55 
.50 
.53 
.51 
.49 

.51 
. !l 
.52 

.53 
.31 

.46 
.37 

.48 

.10 

. 17 



Per cent. 
0.55 
.54 
.54 
.54 
.54 

.50 
.51 
.51 

.53 
.34 

.46 
.10 

.48 
.42 
.-17 



i U. S. Dept. Agr., Bur. Chem. Bui. 107, Bev., p. 41. 

» U. S. Dept. Agr., Bur. Chem. Bui. 107. Rev., p. 241. 

»U. S. Dent. Agr., Bur. Chem. Bui. 134, pp. 16-17. 

« Average figures. 

» Temperature much higher than in the first two experiments. 



MAPLE SUGAR. 9 

In experiments 1 and 2 the results of burning in the three different 
ways are the same when the heat is low. When, however, the heat 
is increased, the percentage drop is 0.05 per cent in experiment 1 and 
0.07 per cent in experiment 2, but the addition of ammonium car- 
bonate brings the results back to the normal. In these two cases the 
extra heating has caused the formation of the oxid from the carbon- 
ate, but has not volatilized any of the ash. Repeating experiment 1 
with a much greater heat, the ash drops 0.22 per cent and comes back 
only 0.03 per cent when moistened and reburned. Similar results 
were obtained in experiments 4 and 5, in both of which the percent- 
age of ash did not come up to the normal by heating with ammonium 
carbonate. All three show the volatilization of some of the ash. 

This all shows the necessity of using the utmost care in carrying 
out this determination. A very dull red is the highest to which an 
ash should be heated; then ammonium carbonate should be added 
and the dish reheated for true results. 

LEAD NUMBER. 

Two determinations of the lead number were made, using basic 
lead acetate solution in both. The lead number using normal lead 
acetate, as described in Bureau of Chemistry Bulletin 134, page 17, 
was not determined on these samples. The ordinary Winton lead 
number determination * was made and also the modification by S. H. 
Ross, 2 which is as follows: 

Transfer 25 grams of the sirup to a 100 cc flask, using about 25 cc of distilled water; 
add 10 cc of potassium sulphate solution (7 grams per liter), 3 then 25 cc of lead sub- 
acetate solution of the strength specified by Winton. Make up to the mark, shake 
thoroughly, and allow to stand 3 hours. Filter, rejecting the first portion of the fil- 
trate. Pipette off 10 cc of the clear filtrate into a 250-cc beaker, dilute to 50 cc, add 
2 cc of 20 per cent sulphuric acid and 100 cc of 95 per cent alcohol. Let stand over- 
night, filter off the lead sulphate on an ignited, weighed Gooch crucible, wash with 
95 per cent alcohol, dry, ignite at low redness for 3 minutes in a muffle or over a burner, 
taking care to avoid reducing cone of the flame, and weigh. Run a blank in exactly 
the same way, substituting 25 grams of a pure cane sugar sirup (66 per cent sucrose 
content) in place of the sirup to be tested. 4 Subtract the weight of the lead sulphate, 
obtained from 10 cc of the sirup test filtrate, from that obtained from 10 cc of the 
cane sugar sirup blank filtrate. The remainder, expressed in grams and multiplied 
by 27.325, gives the modified Winton lead number. 

In both of these tests the composition of the lead subacetate solu- 
tion is of the greatest importance, as it greatly influences the lead 
number. The average results of the basic lead acetate and normal 
lead acetate lead number taken from the work on sap sirups, 5 2.70 

J U. S. Dept. Agr., Bur. Chem. Bui. 134, p. 17. 
* U. S. Dept. Agr., Bur. Chem. Cir. 53. 
8 Freshly boiled distilled water should be used throughout. 

< Do not use acetic acid in this blank; acidified blank is suggested for use only with original Winton 
method. 
6 U. S. Dept. Agr., Bur. Chem. Bui. 134, p. 89. 

61390°— 17— Bull. 466 2 



10 



BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 



standing for the basic solution and 0.79 for the normal lead, indicate 
what may happen when the basicity of the acetate is changed. 
Browne has called attention to the fact that the basicity of the lead 
acetate affects the polarization and also that by digestion of varying 
amounts of neutral lead acetate and litharge at least three well-defined 
subacetates may be prepared. 1 Changes in treatment as to tempera- 
ture and length of time of heating and also quantity of the two ingre- 
dients may form any one of these or a mixture of two. 

An attempt was made to prepare solutions of these different basic 
lead acetates by varying the amount of lead oxid and the manner of 
solution as shown in Table VII. After the solutions were made up 
they were diluted to the same Brix as Winton's solution and a layer 
of heavy oil placed on top. The alkalinity and amount of lead 
were determined in each. 

Table VII. — Effect of method of preparation on basicity of lead acetate solution. 



Solu- 
tion No. 



1.. 
2.. 
3.. 
4. . 
5. . 
6.. 
7.. 
8.. 



Lead 
acetate. 



Grams. 
37.9 
37.9 

75.8 



Litharge. 



Grams. 
22.3 
44.6 
22.3 



Water. 



Cc. 



330 
330 
330 



Solution treatment. 



Home's dry lead subacetate dissolved 



Stood a week; shaken. 

Solution lost 

Stood a week; shaken. 



43.0 


13.0 


1,000 


37.9 


22.3 


330 


75.8 


22.3 


330 



Boiled half hour. 

Do 

Do 



Neutral lead acetate, saturated solution. 



Brix 
reading. 



Degrees. 
15.60 



15.80 
15.60 
16.20 
15.77 
15.87 
15.87 



Nitric 
acid. 



Cc N/10 
acid per 
10 cc. 
30.15 



18. ?5 
26.25 
26.00 
27.50 
19.60 
2.00 



Lead. 



Per cent. 
5.70 



Grams per 
2.5 cc. 
0.1426 



.1398 
.1454 
.1421 
.1449 
.1433 
.1359 



The lead numbers of six samples of maple sirup were determined, 
using these seven solutions. The results appear in Table VIII. 

Table VIII.— Effect of basicity of lead acetate solutions upon the lead number. 



Sample No. 


Lead solution number. 


1 


3 


4 


5 


6 


7 


8 


1 


1.49 
1.74 
1.79 
1.61 
2.00 
1.86 


1.13 
1.34 
1.41 
1.29 
1.47 
1.40 


1.29 
1.42 
1.57 
1.37 
1.64 
1.58 


1.31 
1.51 
1.56 
1.46 
1.70 
1.63 


1.40 
1.62 
1.72 
1.55 
1.80 
1.78 


1.13 
1.27 
1.39 
1.26 
1.41 
1.47 


0.29 


2 


.36 


3 


.36 


4 


.34 


5 


.39 


6 


.37 






Average 


1.75 


1.34 


1.48 


1.53 


1.64 


1.32 


.35 







Solution 4, the one usually employed, consisted of 3 parts of lead 
acetate to 2 parts of lead oxid. Solution 5 was carefully prepared 
by a method that should give this acetate. The results obtained 
from solutions 4 and 5 agree fairly well, the difference between the 
averages being only 0.05 



Solutions 1 and 6 give residts that are 



i U. S. Dept. Agr., Bur. Cheni. Bui. 122, p. 223. 



MAPLE SUGAR. 11 

much above the true lead number, while solutions 3 and 7 are below 
the true results. Solutions 1 and 6 contain more litharge in pro- 
portion to lead acetate than solutions 3 and 7, and likewise show 
a greater alkalinity. The alkalinity of the solution plays an im- 
portant part, for when there is practically no alkalinity, as in No. 
8, the lead number drops to an average of 0.35. 

By preparing the solution of basic lead acetate strictly according 
to the method outlined in Bureau of Chemistry Bulletin 107, Revised, 
or in Winton's original method, or by solution of Home's dry lead 
subacetate, the results of analysis should be comparable and easily 
duplicated. The acidity of the sample itself has little effect on the 
lead number, as shown in Table IX. 

Table IX. — Winton lead number of sirup before and after neutralization. 

[Not calculated to dry basis.] 



Sample. 



Straight sirup 

Sirup after neutralization . 



No. 8451. 



1.75 
1.78 



No. 9235. 



1.49 
1.56 



In both samples the lead number was determined on the original 
sample and again on the same sample after neutralizing the acidity 
with tenth-normal potassium hydroxid, using phenolphthalein as 
an indicator. The acidity in one case, No. 8451, equaled 1 cc, in 
the other, No. 9235, 3 cc, of the tenth-normal potassium hydroxid 
to 100 cc. The neutralization increased the lead number by only 
0.03 and 0.07, respectively. 

MALIC ACID VALUE. 

The calcium acetate method proposed by Cowles * was used for 
this determination. In the Bureau's previous work, it had been found 
that the blanks with calcium acetate were more even and the pro- 
cedure indicated for this method gave a good precipitate which 
settled easily. The procedure is as follows: 

Weigh 6.7 grams of the sample in a sugar dish, transfer to a 200-cc beaker with 
5 cc of water, add 2 cc of a 10 per cent calcium acetate solution, and shake. Stir 
in 100 cc of 95 per cent alcohol and warm the solution until the precipitate settles, 
leaving the supernatant liquid clear. Filter off the precipitate and wash with 75 
cc of 85 per cent alcohol, dry the filter paper, and ignite in a platinum dish. Add 
10 cc of tenth-normal hydrochloric acid and warm gently until all the lime dissolves. 
Cool and titrate back with tenth-normal sodium hydroxid, using methyl orange as 
an indicator. One-tenth of the number of cubic centimeters of tenth-normal acid 
is the malic acid value. Run a blank determination with each set of determina- 
tions, using the same amount of reagents, and subtract the result obtained from 
the malic acid number. 

i Jour. Amer. Chem. Soc, 30 (1908), p. 1285. 



12 BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 

TANNIN REACTION. 

A test for the presence of tannin was made in all of the samples 
by the ferric chlorid reaction as described in Bureau of Chemistry 
Bulletin 134, page 18. 

RESULTS OF ANALYSIS. 

The results of analysis of the samples, given in Table X, are 
arranged by States and counties. The location of the county in 
the State is shown by the usual symbols, namely, □ center, -Q west 
of center, J3 southwest of center, etc. The results of the chem- 
ical examination have been calculated to the dry basis for better 
comparison. Averages have been made for the samples from the 
individual States, from Canada, and from the United States as a 
whole, as well as for all of the samples collected. 



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MAPLE SUGAR. 



27 



DISCUSSION OF RESULTS. 



COLOR. 



Sugar. — The color of a maple sugar, although not necessarily an 
indication of its quality, is influenced by the crystallization and by 
the dryness of the sugar. Very dark maple sirup, if free from sedi- 
ment, when boiled down nearly to dryness and stirred gives a very 
light-colored sugar. If this sugar is powdered, the color and appear- 
ance are similar to those of the ordinary powdered cane sugar, although 
it possesses a maple flavor. Such sugar can also be produced with 
greater ease from a light-colored sirup. The color of the sugars varies 
from 8, the darkest, to 21, the lightest, the average of the indi- 
vidual States showing slight variations from 12 to 15. No compari- 
son has been made between the Canadian and the United States 
samples. 

Sirup. — The average color of the United States sugar-sirup samples 
is 11, which is three points darker than that of the sap sirups. Table 
XI shows the average color of the sugar sirups as well as that of the 
sap sirups for the several States. 

Table XI. — Average color of sugar sirup and sap sirup, by States. 



State. 



Indiana 

Maine 

Maryland 

Massachusetts . . . 

Michigan 

New Hampshire. 



Sugar 


Sap 


sirup 


sirup. 1 


10+ 


10+ 


11 


8+ 


11 


( 2 ) 


9 


7 


11 


8+ 


10 


8 

1 



State. 



New York 

Ohio 

Pennsylvania . 

Vermont 

West Virginia. 
United States. 



Sugar 
sirup. 



10 
10 
11 
11 
12 
11 



Sap 
sirup. 1 



9 
9 

8+ 



1 U. S. Dept Agr., Bur. Chem. Bui. 134. 



No sample. 



In only one State, Indiana, is the color of the sap sirup equal to the 
sugar sirup, there being in all others a difference of at least two 
points. 

TASTE. 



The flavor of a maple product is an indescribable property. It 
is usually possible for a person with an acute sense of taste to differ- 
entiate between sap sirup and sugar sirup after a very few trials. 



SUCROSE. 

The average percentage of sucrose in the sugars when reduced to 
the dry basis is 91.89, with extremes of 98.62 and 57.04. About 
55 of the 283 samples from the United States molded in storage 
before analysis and in a few cases started to ferment. If the ana- 
lytical results on these had been excluded, the average percentage of 
sucrose would be 94.36 instead of 91.89. For sap sirups the average 
figure for sucrose when calculated to dry basis is 95.18 per cent. 



28 



BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 



INVERT SUGAR. 

The extreme percentages of invert sugar in the United States are 
37.30 and 0.09, with an average percentage of 5.46, which would be 
3.09 per cent if the results of the moldy sugar were not included. This 
increase, about 50 per cent higher than in the case of sap sirups, occurs 
because of the inversion of sucrose due to the extra concentration and 
heat when a sap sirup is made into a sugar. About 30 per cent of 
the samples have less than 1 per cent of invert sugar, whereas 53 per 
cent of corresponding samples of sap sirup have less than 1 per cent 
of invert sugar. 

Table XII shows that where large quantities of reducing sugars 
are present in maple sugar the sucrose equivalent of 1 per cent 
reducing sugar is 0.30, which is very close to that of true invert sugar 
of equal parts of dextrose and levulose, but where small percentages 
of reducing sugars are present, there seems to be a large excess of 
levulose, and in many cases a levorotatory substance other than 
levulose is indicated. This was also noted with sap sirup. 1 

Table XII. — Comparison of morose equivalents of 1 per cent of reducing sugar when 

large and small amounts are present. 



Serial No. 


Reducing 
sugar cal- 
culated as 
invert. 


Difference 
in d-'rect po- 
larization 
and in 
sucrose 
by Clerget. 


Sucrose 
equivalent 
of 1 per 
cent re- 
ducing 
sugar. 


Large amounts of reducing sugar: 

6459. 


Per cent. 
9.61 
7.83 
9.49 
7.70 
7.19 

14.27 
6.92 

11.54 
7.27 
8.25 

0.66 
.41 
.58 
.75 
.22 
.65 
.66 
.96 
.78 
.51 


3.46 
3.35 
4.52 
3.94 
3.71 
6.16 
3.00 
5.28 
3.02 
2.20 

2.67 
2.57 
2.77 
2.07 
1.84 
1.00 
2.02 
1.70 
1.S0 
1.30 


0.37 


6545 


.43 


6598 


.47 


6624 


.51 


6700 


.51 


6718 


.43 


6876 - 


.43 


6968 


.46 


8438 


.41 


8446 


.26 


Small amounts of reducing sugar: 

7510 


4.04 


7518 


6.26 


7525 


4.77 


7546 


2.76 


7548 


7.37 


8344 


1.54 


8448 


3.06 


8472 


1.77 


8457 


2.31 


8462 


2.5* 







ASH. 

Total ash. — In the United States samples the average ash content 
is 0.95 per cent, with extremes of 1.66 and 0.76 per cent, while with 
Canada included the average is 0.98 per cent, with extremes of 1.70 
and 0.76. The average for sap sirups for the United States is 1.02 
per cent, with extremes of 1.68 and 0.68. Including Canada, the 

i U. S. Dept. Agr., Bur. of Chem. Bui. 134. p. 65. 



MAPLE SUGAR. 



29 



average is 1 per cent, with the same extremes. Grouping the indi- 
vidual determinations for ash by States and by 0.05 and 0.1 per cent 
differences, the results in Table XIII are obtained. 

Table XIII. — Total ash content of sugar, by locality. 





Number of samples. 


Per- 
cent- 


Ash content. 


Ind. 


Me. 


Md. 


Mass. 


Mich. 


N.H. 


N.Y. 


Ohio. 


Pa, 


Vt. 


W. 

Va. 


Can- 
ada. 


Total. 


age of 
sam- 
ples. 


Per cent. 
0.00 to 0.76 
















'I 
2 
5 
3 
7 
6 
2 
3 
1 








i 1 

3 

7 

7 

7 

10 

11 

15 

9 

4 

3 

2 

31 


2 

33 

56 

39 

56 

51 

48 

36 

22 

6 

9 

3 

2 


0.7 


.77 to .79 




1 

1 
2 


1 

3 
1 
3 
1 


1 

4 
4 
5 


4 
4 
2 
6 
4 
2 
1 


4 
2 
3 
2 

1 


7 

5 

12 

11 

9 

10 

1 
1 


7 
8 
2 
4 
4 
5 
8 
5 


8 
19 
7 
7 
6 
9 
2 
4 


1 
1 

1 
3 


9.1 


.80 to .84.... 

.85 to .89 

.90 to .94.... 

.95 to .99.... 

1.00 to 1.09 


1 
2 
3 
3 
3 
3 
2 


15.4 
10.7 
15.4 
14.0 
• 13.2 


1.10 to 1.19.... 
1.20 to 1.29 




2 


9.9 
6.0 


1.30 to 1.39 












1.6 


1.40 to 1.49 


1 
1 












1 


1 


2.5 


1.50 to 1.59 














.8 


1.60 to 1.70 
















21 


.7 




















Total.... 


19 


4 ! 11 

| 


14 


23 


12 


56 


31 


« 


63 


7 


80 


363 


100.0 



i 0.76. 



2 1.66. 



3 1.70. 



The largest number of samples have a content of ash ranging from 
0.80 to 1.10 per cent, and nearly 88 per cent of the samples range 
from 0.77 to 1.20 per cent. The lowest ash content found in this 
examination, 0.76 per cent, was obtained in a sample from Ohio and 
in one from Canada. In some of the experimental work, however, 
ash contents as low as 0.72 per cent were found. These total ash 
figures may be considered abnormal, as they were found in sirup the 
lead number, malic acid value, and insoluble ash content of which 
were far above the minimum figures. 

Table XIV. — Comparison of percentage of samples of sap and sugar sirup with vary- 
ing ash content. 



Ash content. 


Maple- 
sap 
sirup. 


Maple- 
1 sugar 
sirup. 


Ash content. 


Maple- 
sap 
sirup. 


Maple- 
sugar 
sirup. 


Per cent. 
0.00 to 0.76 


Per cent. 
0.2 
3.7 
11.2 
11.0 
17.7 
12.4 
19.8 


Per cent. 
0.7 
9.1 
15.4 
10.7 
15.4 
14.0 
13.2 


Per cent. 
i 1.10 to 1.19 


Per cent. 

12.3 

6.0 

3.7 

.4 

.6 

1.0 


Per cent. 
9.9 


.77 to .79 


1.20 to 1.29 


6.0 


.80 to .84 


1.30 to 1.39 


1.6 


.85 to .89 


1.40 to 1.49 


2.5 


.90 to .94 


1.50 to 1.59 


.8 


.95 to .99 


1.60 to 1.70 


.7 


1.00 to 1.09 











The same percentage (88.4) of samples in both kinds of sirup have 
ash contents up to 1.20 per cent, although 36 per cent of the sugar 
samples and 26 percent of the sap sirups have an ash content between 
0.77 and 0.89 per cent. The appearance of the ash was not regular, a 
few samples being very green, while many were white or fight gray. 
The appearance of the ash depends upon the method of burning. 



30 



BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 



Soluble and insoluble ash. — The insoluble ash in the United States 
samples shows an average figure of 0.33 per cent, with extremes of 
0.81 and 0.21 per cent, but when Canada is included, the average 
figure is 0.36 per cent, with extremes of 1 and 0.21 per cent. 
These again are somewhat lower than the figures obtained for sap 
sirup. One sample from Michigan, one from Ohio, and one from 
Pennsylvania had only 0.22 per cent of insoluble ash, and another 
from Pennsylvania had 0.21 per cent. The total ash in each of these 
instances was not low, but was near the minimum line. The results 
obtained by grouping the samples by localities and dividing the 
insoluble ash contents into classes by 0.10 per cent are given in 
Table XV. 



Table XV. — Insoluble ash content of sugar, by locality. 





Number of samples. 


Per- 
cent- 


Insoluble 
ash content. 


Ind. 


Me. 


Md. 


Mass. 


Mich. 


N.H. 


N.Y. 


Ohio. 


Pa. 


vt. 


W.Va. 


Can- 
ada. 


Total. 


age 
of 

sam- 
ples. 


Per cent. 
Below 0.23... 










i 1 

8 
6 
7 
1 






i 1 
6 
5 

17 
2 


22 

4 
14 
14 
6 
2 
1 








4 

35 

112 

112 

49 

24 

17 

6 

3 


1.4 


0.23 


4 
5 
4 
2 
3 


1 
1 
2 


1 

5 
4 
1 


4 
8 
2 


6 
5 
1 


7 

29 
15 

4 








9.6 


.24 to 0.29... 
.30 to .39... 
.40 to .49... 
.50 to .59... 


18 
24 

7 
8 
5 


3 
2 
2 


15 

18 
22 
9 
8 
5 
2 


30.8 

30.8 

13.5 

6.6 


.60 to .69... 












1 




4.7 


.70 to .79... 


1 












1.6 


.80 to .89... 


















.. 3 1 




0.8 


.90 to .99... 
























1.00 to 1.09... 
























<1 


1 


0.2 




























Total.. 


19 


4 


11 


14 


23 


12 


56 


31 


43 


63 


7 


80 


363 


100.0 



i 0.22. 



2 0.21, 0.22. 



3 0.81. 



* 1.00. 



From this it is seen that 72.6 per cent of the samples have an 
insoluble ash content of less than 0.40 per cent. In Canada 59 per 
cent of the samples have a higher number than that, while all the 
West Virginia samples have a higher insoluble ash content than 
0.40 per cent. The other States show their largest figures below 
0.40 per cent. 

Percentage of soluble ash divided by percentage of insoluble ash. — The 
average figure is 1.69; that is, the percentage of insoluble ash is 
about 55 per cent of the soluble ash. The highest is 4.07 and the 
lowest, 0.43. Among the sap sirups some 29 samples, or 6 per cent, 
showed a ratio below 1.0; among the sugar sirups 8 per cent were 
found with this low ratio. These samples were confined to the 
State of Vermont and to Canada. From Table XVI, showing the 
data by groups of 0.01 and 0.25, it is seen that the largest percent- 
age of samples falls between 1.25 and 2.75. 



MAPLE SUGAR. 31 

Table XVI. — Soluble and insoluble ash content of sugar, by locality. 



Soluble ash 


Number of samples. 


Per- 

eenl- 


divided by 
insoluble ash. 


Ind. 


Me. 


Md. 


Mass. 


Mich. 


N.H. 


N. Y. 


Ohio. 


Pa. 


Vt. 


W. Va. 


Can- 
ada. 


Total. 


age 
of 
sam- 
ples. 


Per cent. 
0.0 to 0.59. . . 
























12 
1 
6 
3 
4 

13 

13 
8 
8 

10 
4 
7 


2 

3 

10 

8 

6 

33 

46 

38 

37 

54 

47 

43 

18 

14 

3 

1 


0.7 


.60 to .69... 




















2 
4 
5 
2 
7 
6 

12 
9 

10 
5 


5' 

1 

1 


.8 


.70 to .79... 




















2.7 


.80 to .89... 




















2.2 


.90 to .99... 




















1.6 


1.00 to 1.24... 


3 
1 
1 




2 






1 
4 

1 
2 
1 
3 


3 
7 
3 
7 
6 
8 

12 
5 
3 
1 

2 1 


3 
1 
5 
3 
5 
5 
7 
1 
1 


1 
8 
6 
2 
9 
10 
3 
3 


9.1 


1.25 to 1.49... 




1 
3 
3 
3 
4 
4 
1 
4 


12.7 


1.50 to 1.74. . . 








10.4 


1.75 to 1.99... 


1 
1 
2 


2 
3 
3 
1 


2 
1 
3 
3 
5 


10.2 


2.00 to 2.24... 
2.25 to 2. 49... 
2.50 to 2. 74... 


2 
4 
3 
4 


14.8 
13.0 
11.8 


2.75 to 2.99,. . . 


1 




5.0 


3.00 to 3.49... 








1 


3.8 


3.50 to 3.99... 


1 






1 






.8 


4.00 to 4. 10... 


















.4 






























Total.. 


19 


4 


11 


14 


23 


12 


56 


31 


43 


63 


7 


80 


363 


100.0 



1 0.43, 0.57. 



2 4.07. 



Alkalinity of soluble and insoluble ash. — This determination is ex- 
pressed in the number of cubic centimeters of tenth-normal acid neces- 
sary to neutralize the ash of 100 grams of sirup. For insoluble ash, 
which is chiefly calcium carbonate, the average figure is 87 cc, the ex- 
tremes being 190 and 31. Since 1 cc of tenth-normal acid is equal to 
0.005 gram of calcium carbonate, the 87 cc are equivalent to 0.435 gram 
of calcium carbonate. The actual average percentage of insoluble 
ash is 0.36, which is 0.07 gram lower than that calculated from the 
alkalinity. The average figure for soluble ash is 75 cc, with extremes 
of 140 and 42. Considering the soluble ash to be potassium carbon- 
ate, the 75 cc would equal 0.518 gram of potassium carbonate. The 
average percentage of soluble ash is 0.62, which is 0.11 gram higher 
than that calculated from the alkalinity. This may be accounted 
for by the presence of alkaline salts other than potash. 



LEAD NUMBER. 



The average lead numbers for the individual States vary to a 
great extent, as shown in Table XVII : 

Table XVII. — Average of the Winton and Ross lead numbers, by States. 



No. 



Locality. 



Winton 

lead 
number. 



Locality. 



Ross 

lead 

number. 



West Virginia . . . 

Indiana 

Canada 

Pennsylvania . . . 

Ohio 

Vermont 

Massachusetts . . . 

Maryland 

Michigan 

New Hampshire . 

Maine 

New York 



3.99 
3.04 



West Virginia . 
Indiana 



Pennsylvania . . . 

Ohio 

Vermont 

Massachusetts.. . 

Maryland 

Michigan 

New Hampshire . 

Maine 

New York 



4.49 
3.73 



0) 



3.34 
3.29 



.39 
.35 
.99 
.33 
.50 
3.40 
3.05 



1 Canada is not included, as this determination was not made on all the samples. 



32 



BULLETIN 466, U. S. DEPAETMENT OF AGRICULTURE. 



West Virginia and Indiana stand at the top in each determination* 
the rest of the localities varying in their places. It is noted that in 
each case the Ross lead number is higher than the Winton. The 
average for the Winton number in the United States samples is 2.68, 
with extremes of 4.95 and 1.85. Including the results from the 
Canadian samples the average is 2.76, with the same extremes. 
With the Ross number, the United States average is 3.34, with 
extremes of 5.90 and 2.20. The increase in lead number by the 
Ross method averages 0.58. 

Grouping the lead number by localities into divisions varying by 
0.25 and placing the samples with these figures in such groups, the 
results in Table XVIII are obtained. 



Table XVIII. — Lead number of sugar , by locality. 













N 


mnber of samples. 












Per- 
cent- 


Lead number. 


Ind. 


Me. 


Md. 


Mass. 


Mich. 


N.H. 


N.Y. 


Ohio. 


Pa. 


Vt. 


W. 
Va. 


Can- 
ada. 


Total. 


age 
of 
sam- 
ples. 


Winton: 

0.00 to 1.84.. 





























1.85 to 1.99.. 










3 
4 
6 
3 
3 
2 
2 


2 
1 
5 
1 
2 

1 


3 
16 

16 

14 

4 

1 

1 


2 
7 
3 
6 
3 
3 
2 
3 
1 
1 


4 
9 
6 
2 
4 
6 
1 
4 
5 
2 


7 
11 
12 
5 
6 
5 
7 
6 
2 
1 


1 
1 
1 

2 
2 


1 

3 

15 

10 

7 

15 

14 

8 

4 

3 


22 
56 
74 
49 
38 
41 
30 
24 
12 
11 
2 


6 1 


2.00 to 2.24.. 
2.25 to 2.49.. 
2.50 to 2.74.. 
2.75 to 2.99.. 
3.00 to 3.24.. 
3.25 to 3.49.. 


1 
1 

4 
5 
3 
1 
1 
1 
2 


2 
1 


3 
3 
1 
1 

3 


1 
5 
2 
3 
2 
1 


15.5 
20.5 
13.6 
10.5 
11.3 
8.3 


3.50 to 3.74.. 






6.6 


3.75 to 3.99.. 


1 










3.9 


4.00 to 4.49. . 












3.1 


4.50 to 5.00.. 














0.6 


























Total 


19 


4 


11 


14 


23 


12 


*55 


31 


43 


162 


7 


89 


361 


100.0 


Ross: 

0.00 to 2.24.. 
















1 
2 
3 
4 
4 
5 
6 
4 


1 
4 
6 
10 
1 
3 
6 
2 
2 
4 
2 
2 


1 
2 

7 
7 

13 
6 
5 

11 
6 
2 
3 






3 
13 

29 

40 

50 

42 

39 

28 

14 

10 

9 

3 

1 


1.1 


2.25 to 2.49.. 






2 
2 
1 
3 
1 
1 
1 








3 

7 

14 

15 

10 

3 

2 






4.6 


2.50 to 2.74. . 




.1 


1 

3 
6 
3 
1 


1 
3 
6 
6 
4 
1 
2 


1 
1 
1 

4 

3 






10.3 


2.75 to 2.99.. 








14.2 


3 00 to 3.24 


4 








17.8 


3.25 to 3.49.. 


1 
1 




14.9 


3.50 to 3.74.. 
3 75 to 3 99 


8 
2 
3 


2 

1 


13.9 
10.0 


4.00 to 4.24.. 


1 
1 
1 
1 

1 




5.0 


4.25 to 4.49.. 








2 




i 

1 


3.6 


4.50 to 4.74.. 


2 










3.1 


4.75 to 4.99 














1.1 




















0.4 


























Total 


19 


4 


11 


14 


23 


12 


'-'54 


31 


43 


63 


7 




281 


100.0 



1 Determinations not made on one sample. 



2 Two not made. 



In the total column of the Winton 'number, most of the sam- 
ples have a number between 2.00 and 3.50. In some States 
the variation is rather small; for example, New York shows 83 per 
cent of samples between 2.00 and 2.74, Indiana 70 per cent of sam- 
ples between 2.50 and 3.24 while in West Virginia no samples were 
found with a number below 3.00. 

With the Ross number the largest percentage of samples falls be- 
tween 2.50 and 3.99, New York showing 72 per cent between 2.75 



MAPLE SUGAR. 



33 



and 3.49, Indiana nearly 50 per cent of samples with a lead number 
between 3.50 and 3.74, and West Virginia no samples below 3.25. 

Boss * indicates that the excess of both lead subacetate and sugar 
exert a marked effect upon the lead subacetate precipitate and shows 
that the effect of the excess of sugar is relatively greater. In the 
procedure for his method potassium sulphate is added to the solu- 
tion before the lead subacetate to overcome the solvent action of the 
sugar upon the lead precipitate. Ross believes this solvent action 
to be the cause of the lead number of mixtures of maple and cane 
sirup not being proportional to the percentage of maple present. 
The figures by Ross lead number given herein, however, apply only 
to sirups having a density of approximately 65 per cent solids which 
were made up from pure maple sugar, and the application of lead 
number determinations to mixtures of maple and cane sugar sirup 
has not been entered into in connection with this bulletin. In 
Table XIX the increase of the individual samples is grouped by 
differences of 0.10 and by States. 



Table XIX. — Differences between Winton and Ross lead numbers. 




Lead number. 


Number of samples. 


Per- 
cent- 
age of 
sam- 
ples. 


Ind. 


Me. 


Md. 


Mass. 


Mich. 


N.H. 


N.Y, 


Ohio. 


Pa. 


Vt. 


w. 

Va. 


Total. 


Winton higher than 
















2 








2 
1 
9 

10 

13 

20 

34 

37 

31 

40 

37 

24 

7 

8 

3 

3 

1 


0.7 


Winton and Ross 


















1 

1 

3 

8 

11 

6 

12 

10 

6 


1 

1 
1 
2 
1 

1 


.3 


Ross higher by less 
than 0.10 














1 


3 

2 
3 
2 
1 
1 
4 
4 
3 
4 
1 
1 


4 

4 
2 
4 

8 
8 
5 
4 
1 
1 


3.2 


Ross higher by more 
than: 
0.10.. . 


1 




2 
3 
2 
1 
2 








3.6 


.20 


1 
1 
1 
3 
2 
2 
1 
1 
1 
1 






2 

5 

11 

10 

7 
5 

7 

2 
3 


4.6 


.30 






1 




7.1 


.40 


2 


1 


12.2 


.50 


2 
4 
6 
5 
3 
2 


3 
3 

4 

1 


13.2 


.60 


3 
4 
6 
2 
1 




11.1 


.70.., 






14.3 


.80 


1 
1 


1 


13.2 


.90 


8.6 


1 00 


2.5 


1.10 








2 
2 




2.9 


1.20 . 




1 




1.1 


1 30 










1 


1 




1 
1 


1.1 


1.40 
















.3 


























Total 


19 


4 


11 


14 


23 


12 


54 


31 


43 


62 


7 


280 


100.0 






Difference: 

Average 

Maximum . , . 
Minimum 


69 
112 

48 


93 

126 

49 


38 
92 
16 


68 

116 

29 


81 

104 

35 


100 
133 

74 


63 
137 

8 


55 
121 


50 

142 

3 


69 
129 


50 

95 

6 



















The increase varies greatly in the samples, the greatest increase 
being 1.42 and the least 0.15. Eighty per cent of the samples show 
an increase of from 0.30 to 1. Table XX gives the results of samples 
that show little difference between the two numbers, from which 
it is seen that factors other than the solubility of the lead precipitate 
in the sugar solution enter into the amount of the lead number. 

i U. S. Dept. Agr., Bur. Chem. Cir. 53. 



34 BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 

Table XX. — Samples with Winton and Ross lead numbers showing slight variation. 



State. 


Serial No. 


Lead numbers. 


Winton. 


Ross. 


Difference. 


Ohio 


6315 
6318 
6788 
7561 
6313 
6373 
6374 
6882 
6884 
6864 
6872 
7503 


3.61 
3.47 
3.58 
2.37 
3.53 
2.16 
2.23 
3.22 
2.77 
3.68 
3.69 
4.64 


3.57 
3.32 
3.58 
2.45 
3.62 
2 22 
2.25 
3.30 
2.86 
3.71 
3.74 
4.70 


—0.04 


Do 


- .15 


Vermont 


.00 


New York 


+ .08 


Ohio 


+ .09 


Do 


+ .06 


Do 


+ .02 


Pennsylvania 


+ .08 


Do 


+ .09 


Do 


+ .03 


Do 


+ .05 


West Virginia 


+ .06 






MALIC ACID 


VALUE. 









The average of all determinations was 0.93, with extremes of 1.72 

and 0.51. This average is a little below that obtained on sap sirups, 

1.01, and the extremes are not as far apart as in sap sirups. The 

results by localities and groups of 0.10 and 0.25 are tabulated in 

Table XXI. 

Table XXI. — Malic acid value of sugar, by locality. 



Malic acid 


• . Number of samples. 


Per- 
cent- 
age of 
sam- 
ples. 


value. 


Ind. 


Me. 


Md. 


Mass. 


Mich. 


iN.H. 


N.Y. ' Ohio. 


Pa. 


Vt. 


W. 

Va. 


Can- 
ada. 


Total. 


0.00 to 0.59 


















il 
3 
7 

16 

14 

2 


21 

8 

7 

26 

19 

2 






2 

26 

59 

143 

105 

23 

4 


0.7 


.60 to .69 




1 
3 


1 
5 
3 
2 


1 
9 
4 


6 

2 

12 

3 


4 
4 
4 


3 

14 

30 

9 


2 

8 
7 

12 
1 


2 
2 
3 


2 

9 

25 

29 

14 

1 


7.2 


.70 to .79.... 

.80 to .99 

1.00 to 1.24.... 
1.25 to 1.49 


2 

8 
7 
2 


16.3 

39.2 

29.0 

6.3 


1.50 to 1.74 














1.3 
























Total... 


19 


4 


11 


14 


23 


12 


56 3 30 


43 


63 


7 


80 


3 362 


100.0 



i 0.59. 



2 0.51. 



3 One missing. 



The largest number of samples falls in the groups from 0.70 to 
1.24. Two samples show figures below 0.60, one from Pennsylvania 
with a value of 0.59, and one from Vermont with a value of 0.51, 
while in the sap sirup 6 out of the 480 showed values below 0.60, 
one being as low as 0.21. 

TANNIN REACTION. 

The ferric-chlorid test showed indications of tannin in nearly one- 
third of the samples, being very strong in 10 samples. In all cases 
where tannin was noted the color of the sirup was dark, and in most 
of these the flavor was poor. The fact that tannin was found in a 
larger number of the sugar-sirup samples than of the sap-sirup sam- 
ples may be accounted for by the fact that less care was taken in the 
preparation of the maple sugar than in that of the sap sirup. Many 



MAPLE SUGAK. 



35 



tests have been made of the fresh sap in different bushes with ferric 
chlorid, but in no case has a coloration due to tannin been noted. 
Tannin is present in sap that has stood during a rainstorm, as well 
as in dirty sap. 

UNDETERMINED MATTER. 

As this is a difference figure, it is influenced by the accuracy of the 
other determinations. The highest figure noted for the United States 
samples was 5.84, and the minimum was 0, the average being 1.70. 
This difference is almost entirely accounted for when ash, which is 
weighed as a carbonate, is calculated to a malate, in which condition 
it is supposed to occur naturally. 

CANADIAN MAPLE SUGARS. 

Comparison of Canadian sap sirups with those from the United 
States showed that they were darker in color and gave lower ana- 
lytical results. 1 The same comparison on maple sugars shows that 
on an average the analytical figures for Canadian samples are slightly 
higher than those for the United States. Table XXII gives the 
average results. 

Table XXII. — Comparison of analytical results for Canadian and United States sugar. 



Determination. 


United 

States 

samples 

(283). 


Canadian 

samples 

(80). 


Determination. 


United 

States 

samples 

(283). 


Canadian 

samples 

(80). 


Invert sugar do — 

Undetermined do 


91.89 

5.46 

1.70 

.95 


86.48 
8.76 
3.70 
1.06 


Insoluble ash per cent. . 

Soluble ash do 

Winton lead number 


0.33 

.62 

2.68 


0.45 

.61 

3.04 


Total ash do 


Ross lead number 


!3.34 
.91 


2 3. 66 






1.03 


Total do.... 

<• 


100.00 


100.00 
1 





i Average of determinations on 282 samples. 

2 Average of determinations on 26 samples. Determination not made on rest of the 80 samples. 

The darker color of the Canadian samples was due to the process 
of manufacture rather than to the environment or climate, for prod- 
ucts as light colored as those, manufactured in the United States are 
made in Canada. Crudeness in the process leads to dark, strong- 
flavored products, which are of no value for consumption in that 
condition, but find a market in mixtures of maple and sugar sirups 
or for giving flavor to a sirup. 

The Canadian samples may be grouped into three divisions, those 
coming from Beauce and the surrounding townships, those from the 
region below Montreal, centered around Sberbrook and Waterloo, 
and those above Montreal in Joliette Township. Figure 1 shows the 
relative location of these townships, as well as the average figures for 
the important analytical determinations. 

i U. S. Dept. Agr., Bur. Chem. Bui. 134, pp. 75-76. 



36 



BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 



From this it is seen that the figures for the Beauce district are a 
little higher than those for the other two districts, the region below 
Montreal giving the lowest figures and that above Montreal the next 
lowest. This is apparently the direct opposite of the tendency of the 
sugar sirup of the United States. 

EFFECT OF ENVIRONMENT ON THE COMPOSITION OF MAPLE SUGAR. 

In the case of sap sirup, there is a relationship between the loca- 
tion of States and the composition of the product. Taking the 
average determinations for the States and localities in some of the 




Fig. 1. — Map showing effect of environment on analytical results of maple sugar, Canada. 

States, as one goes north there is a lower figure for total ash, lead 
number, and mafic acid value. Tabulating the results of the maple 
sugar work in this way, the same general tendency is noted. 

Table XXIII. — Average analyses of samples, by localities. 



Determination. 


Analyses. 


W.Va. 


Ind. 


Ohio. 


Md. 


Pa. 


Mich. 


Mass. 


NY. 


Vt. 


N.H. 


Me. 


Can- 
ada. 


Sucrose per cent. 

Invert sugar do. . . 

Total ash do. . . 

Insoluble ash do. .. 

Winton lead number 

Ross lead number 


91.15 
6.27 
1.37 
.53 
3.99 
4.49 
1.38 


90.16 
5. 04 
1.08 
.36 
3.04 
3.73 
1.00 


89.98 

6.52 

.95 

.31 

2.74 

3.29 

.92 


95.38 

1.89 

.91 

.31 

2.61 

2.99 

.85 


92.92 

4.92 

.97 

.33 

2.84 

3.34 

.93 


92.00 

4.63 

.90 

.28 

2.52 

3.33 

.83 


93.17 

5.44 

.98 

.26 

2. 67 

3.35 

.99 


96. 04 

2.33 

.92 

.30 

2.42 

3.05 

.87 


88.39 

8.37 

.92 

.38 

2.70 

3.39 

.92 


89.54 

7.71 

.91 

.32 

2.50 

3. 50 

.92 


94.11 

4.06 

.90 

.29 

2.43 

3.40 

.82 


86.48 

8.76 

1.06 

.45 

3.04 


Malic acid value 


1.03 







MAPLE SUGAR. 



37 



The southern maple-producing States, West Virginia, Indiana, 
Ohio, Pennsylvania, and Maryland, show higher figures than the 
northern States, Vermont, New Hampshire, Maine, and Michigan. 
This relationship becomes more evident when the figures are inserted 
in a map of the United States in the region from which the samples 
come. In the western group, West Virginia, Maryland, Pennsyl- 
vania, Ohio, Indiana, and Michigan, the sectional differences are 
very marked. With the exception of the Maryland figures, the drop 
in all determinations as one goes north is very marked. From West 




Fig. 2.— Map showing effect of environment on analytical results of maple sugar, United States. 

Virginia to Michigan there is a drop of 0.47 per cent in ash, of 0.25 
per cent in insoluble ash, of 1.47 in Winton lead number and 1.16 
in Ross lead number, and of 0.55 in the malic acid value. In the 
eastern section, comprising New York, Massachusetts, Vermont, New 
Hampshire, and Maine, the drop as one goes north is not so great. 
From Massachusetts to Maine, the drop in total ash is 0.08 per 
cent, in insoluble ash none, in Winton lead number 0.24, in Eoss 
lead number none, and in malic acid value 0.17. 

It is evident, then, that environment plays some part in the com- 
position of maple sugar. 



38 



BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 



CHANGES IN COMPOSITION AND COLOR FROM SAP SIRUP TO SUGAR 

SIRUP. 

The sirup from maple sugar has a more even color and flavor than 
sap sirup, due to the mixing of various grades of maple sugar. It 
is much darker in color than that of the original sap sirup, and the 
taste is greatly changed, although no comparative figures along this 
line are available. 

Ten samples of the sap sirup were collected and analyzed; a por- 
tion of the sirup was then concentrated in a glass vessel over a lamp 
to the sugaring-off point, stirred, and allowed to cool. The sugar 
so produced was again dissolved in water to the consistency of com- 
mercial sap sirup, filtered, and analyzed. In this additional con- 
centration, in most cases, very little precipitation occurred. There 
was enough, however, to make the sugar sirup cloudy, but this soon 
settled when allowed to stand. For comparison, the figures obtained 
on analysis were calculated to the dry basis. 

Table XXIV. — Changes in color and composition from maple-sap sirup to maple-sugar 

sirup. 



Kind of sirup. 


Color. 


Sucrose. 


Invert 

sugar. 


Ash. 


Insoluble 
ash. 


Lead 
number. 


Malic acid 
value. 






Per cent. 


Per cent. 


Per cent. 


Per cent. 








10 


93.83 


3.68 


0.78 


0.28 


2.19 


0.75 




7 


96.80 


.93 


.84 


.24 


2.26 


.84 




7 


96.64 


.45 


.90 


.23 


2.00 


.77 




9 


95.10 


1.84 


.94 


.40 


2.84 


1.05 




7+ 


95.13 


1.20 


1.07 

.87 


..46 


3.13 


1.16 




9 


95.23 


.71 


.27 


2. 28 


.87 




8 


94.26 


1.43 


.83 


.34 


2.56 


.85 




8 


92.93 


2.63 


.82 


.36 


2.70 


.87 




9+ 


95.15 


.81 


.80 


.26 


1.93 


.69 




8 


95.82 


1.10 


.82 


.23 


1.99 


.73 


Average 


8.2 


95.12 


1.48 


.87 


■ .31 


2.39 


.86 








12 


83.03 


8.86 


.77 


.22 


2.04 


.62 




9 


96.10 


1.51 


.81 


.22 


1.96 


.60 




9 


96.18 


1.07 


.77 


.22 


2.42 


.61 




9+ 


94.18 


3.46 


.80 


.23 


2.07 


.63 


Sugar sirup 


9 
11 


95.24 
94.90 


1.49 
1.40 


.88 
.85 


.22 
.23 


2.20 
2.11 


.66 




.59 




9 


95.60 


1.70 


.79 


.28 


1.98 


.64 




9 


92.88 


3.08 


.80 


.31 


2.?9 


.69 




11 


95. 25 


1.11 


.85 


.22 


1.96 


.69 




9 


96.11 


1.32 


.83 


.23 


2.09 


.74 


Average 


9.7 


93.95 


2.56 


.81 


.24 


2.11 


.65 



Taking the individual determinations as given in Table XXIV, the 
color increases in every case, the average increase being two colors. 
If this concentration had been carried on under commercial con- 
ditions, the color would probably have been influenced to a greater 
extent, for the boiling in this instance was carried on under the best 
possible conditions, in glass apparatus. In concentration, the per- 
centage of sucrose has decreased in nearly all cases, while at the same 
time there is an increase in the percentage of invert sugar, showing 
that longer and higher heating tends to break down the sucrose. 



MAPLE SUGAE. 



39 



The percentage of ash drops ficm 0.87 to 0.81 per cent, and of 
insoluble ash from 0.31 to 0.24 per cent, the lime salts evidently 
being the ones eliminated. The figures for the lead number show a 
decrease of 0.28 from 2.39 to 2.11, and the malic acid value decreases 
from 0.86 to 0.65, all indicating that a malate of lime is precipitated. 

MOISTURE IN MAPLE SUGAR. 

The percentage of moisture was determined in only a few of the 

samples of sugars. The percentage varied somewhat, as shown in 

Table XXV. 

Table XXV. — Moisture in maple sugar. 



Sample No. 



Grain sugar: 

8413 

8338 

8339 

8344 

8333 

Cake sugar: 

8325 

8324 

8349 

8350 

8351 

8387 

8460 

8500 

8372 

8381 

8326 

8327 

8345 

8354 

8355..... 

8356 

8358 

8359 



Condition. 



Mois- 
ture. 



Very dry 

Medium dry. 

do 

....do 

Soft 



Hard 

do 

do 

do 

do 

Very hard 

Hard 

....do 

....do 

....do 

Medium hard. 
....do 



.do. 
.do. 
.do. 
.do. 
.do. 
.do. 



Per 

cent. 
0.65 
3.84 
6.65 
8.42 

11.00 



4.19 
5.28 
8.18 
7.35 
5.87 
1.43 
5.21 
7.40 
3.15 
2.10 
8.88 
9.21 
7.53 
7.79 
8.24 
7.95 
6.97 
6.32 



Sample No. 



Condition. 



Cake sugar- 
8360.... 
8362. . . . 
8364.... 
8366.... 
«367.... 
8375. . . . 
8378. . . . 
8386. . . . 
8430. . . . 
8433.... 
8451.... 
8452. . . . 
8454. . . . 
8501.... 
8346.... 
8347. . . . 

8348 

8352. . . . 
8353.... 
8365. . . . 
8374.... 
8434.... 
8463.... 
8466. ... 



Con. 



Medium hard. 
do 



.do. 
.do. 
.do. 
.do. 
.do. 
.do. 
.do. 
.do. 
.do. 
.do. 
.do. 
.do. 



Soft. 



.do. 
.do. 
.do. 
.do. 
.do. 
.do. 
.do. 
.do. 
.do. 



Mois- 
ture. 



Per 

cent. 

6.28 

6.46 

6.78 

9.67 

7.43 

8.50 

8.31 

5.53 

6.96 

7.08 

7.97 

9.45 

8.57 

6.22 

10.79 

9.64 

10.41 

10.60 

10.40 

10.66 

10.27 

9.88 

11.20 

10.44 



As the percentage of water increases, the cake becomes softer, but 
no exact lines can be drawn on moisture content between soft and 
hard sugar. This depends to a great extent on the moisture content, 
but also on the chemical composition, that is , on the percentage of invert 
sugar. In general, sugars having more than 9 per cent of water are 
soft enough to drain badly. In fact, if most cakes with even 7 per 
cent of water were allowed to stand for some time there would be an 
appreciable quantity of drained molasses. In the 47 samples ex- 
amined, the moisture content varied from 0.65 to 11.20 per cent. A 
former publication 1 gives as the maximum for moisture 1 1 per cent 
and the minimum 3.05 per cent. Hortvet 2 reports samples with 
4.27 to 15.67 per cent of moisture, while McGill 3 reports analyses 
of 83 samples with a moisture content of from 0.06 to 7.06 per cent. 

The method proposed by Stanek 4 with his tables, using an im- 
mersion refractometer, was the one used for this determination. 
The great value of this method lies in its quick and comparable results. 

i U. S. Dept. Agr., Bu. Chem. Cir. 40. 

2 Jour. Amer. Chem. Soc., 26 (1904), p. 1523. 

3 Lab. Inland Rev. Dept. Canada Bui. 258. 

* Zeit. Zuckerind. Bohmen, 35 (1910), p. 57; 35 (1911), p. 187. 



40 



BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 



In this method specially standardized 100 cc flasks are used. 
Upon their necks are etched marks showing where 100 grams of 
recently boiled distilled water reach, at a temperature of 17.5° C. 
The correctness of all readings depends on this graduation. 

Twenty grams of the sample are weighed and transferred with 
water to one of these flasks. The sugar is dissolved by shaking, 
and the flask, after being filled almost to the mark with water, is 
allowed to stand in a constant temperature bath for 20 or 30 minutes 
with occasional shaking. The volume is then completed with water 
of the same temperature, the solution shaken, and a reading taken 
with the immersion refractometer, the temperature being noted at 
the same time with an accurate thermometer (better calibrated to 
one-tenth). If the temperature is any other than 17.5° C, the reading 
obtained must be corrected by the figures opposite the temperature 
in Table XXVI. For readings taken at temperatures below 17.5° C. 
the correction is subtracted, and for readings at temperatures above 
17.5° C. the correction is added. 





Table XXVI. — Temperature corrections. 1 




Tem- 


Num- 
ber to 


Tem- 


Num- 
ber to 


Tem- 


Num- 
ber to 


Tem- 


Num- 
ber to 


pera- 
ture. 


be sub- 
tracted. 


pera- 
ture. 


be 
added. 


pera- 
ture. 


be 
added. 


pera- 
ture. 


be 
added. 


°C. 




° C. 




°C. 




°C. 




15.0 


0.72 


17.6 


0.03 


20.2 


0.82 


22.8 


1.62 


15.1 


.70' 


17.7 


.06 


20.3 


.85 


22.9 


1.65 


15.2 


.67 


17.8 


.09 


20.4 


.88 






15.3 


.64 


17.9 


.12 


20.5 


.91 


23.0 


1.69 


15.4 


.61 






20.6 


.94 


23.1 


1.72 


15.5 


.58 


18.0 


.15 


20.7 


.97 


23.2 


1.75 


15.6 


.55 


18.1 


.18 


20.8 


1.00 


23.3 


1.78 


15.7 


.52 


18.2 


.21 


20.9 


1.03 


23.4 


1.81 


15.8 


.49 


18.3 


.24 






23.5 


1.85 


15.9 


.46 


18.4 


.27 


21.0 


1.06 


23.6 


1.88 






18.5 


.30 


21.1 


1.09 


23.7 


1.91 


16.0 


.44 


18.6 


.33 


21.2 


1.12 


23.8 


1.96 


16.1 


.41 


18.7 


.36 


21.3 


1.15 


23.9 


1.99 


16.2 


.38 


18.8 


.39 


21.4 


1.18 






16.3 


.35 


18.9 


.42 


21.5 


1.22 


24.0 


2.03 


16.4 


.32 






21.6 


1.25 


24.1 


2.06 


16.5 


.29 


19.0 


.45 


21.7 


1.28 


24.2 


2.09 


16.6 


.26 


19.1 


.48 


21.8 


1.31 


24.3 


2.12 


16.7 


.23 


19.2 


.51 


21.9 


1.34 


24.4 


2.15 


16.8 


.20 


19.3 


.54 






24.5 


2.19 


16.9 


.17 


19.4 


.57 


22.0 


1.37 


24.6 


2.22 






19.5 


.61 


22.1 


1.41 


24.7 


2.25 


17.0 


.15 


19.6 


.64 


22.2 


1.44 


24.8 


2.29 


17.1 


.12 


19.7 


.67 


22.3 


1.47 


24.9 


2.32 


17.2 


.09 


19.8. 


.70 


22.4 


1.50 






17.3 


.06 


19.9 


.73 


22.5 


1.53 


25.0 


2.35 


17.4 


.03 






22.6 


1.56 


25.1 


2.38 


17.5 


.00 


20.0 


.76 


22.7 


1.59 


25.2 


2.42 






20.1 


.79 






25.3 


2.45 



i Stanek, Zeit. Zuckerind. Bohmen, 35 (1911), p. 187. 

The percentage of the dry substance is then obtained from Table 
XXVII. 



MAPLE SUGAR. 



41 



Table XXVII. — Dry substance equivalent to temperature corrected immersion refrac- 

tometer readings {20 grams to 100 cc). 1 



Refrac- 

tometer 

reading. 2 


Dry sub- 
stance. 


Refrac- 
tometer 
reading. 2 


Dry sub- 
stance. 


Refrac- 
tometer 
reading. 2 


Dry sub- 
stance. - 


Refrac- 
tometer 
reading. 2 


Dry sub- 
stance. 


°C. 
74.0 
75.0 
7C.0 
77.0 
78.0 


Per cent. 
77.35 
78.60 
79.90 
81.15 
82.40 


°C. 
79.0 
80.0 
81.0 
82.0 
83.0 


Per cent. 
83.70 
84.95 
86.25 
87.50 
88.75 


" C. 
84.0 
85.0 
86.0 
87.0 
88.0 


Per cent. 
90.05 
91. 30 
92.60 
93.85 
95.10 


° C. 
89.0 
90.0 
91.0 
92.0 


Per cent. 

96.35 

97.60 

98.85 

100.00 



i Stanek, Zeit. Zuckerind, Bohmen, 35 (1911), p. 187. 2 Tenths of readings may be interpolated. 

Subtracting the percentage of dry substance from 100 gives the 
percentage of moisture. 

To illustrate the manner of using the tables, 20 grams of sugar 
made up at 15.5° C. gave a reading of 90.15. The correction for 
15.5° C. is 0.58, which subtracted from 90.15 gives 89.57. The dry 
substance for 89.0 is 96.35 per cent and for 90.0 it is 97.60 per cent, 
a difference of 1.25 per cent. Fifty-seven hundredths of 1.25 is 
0.71, which added to 96.35 gives 97.06, the percentage of dry sub- 
stance, or a moisture content of 2.94 per cent. 

Table XXVIII shows that the results by this method approached 
very nearly the results of the usual drying method. 

Table XXVIII — Moisture 'content of sugar by drying and by refractometer . 



Sample No. 


Drying. 


Refracto- 
meter. 


1 


Per cent. 
1.35 

.62 
2.32 

.85 
1.96 


Per cent. 
1.40 


2 . 


.65 


3 


2.40 


4 


.90 


6.... 


2.09 







MAPLE CREAM, HONEY, AND WAX. 

Among the numerous products made from maple sap may be 
mentioned maple cream (or maple butter), maple honey, and maple 
wax. 

Maple cream is produced by boiling the sirup to a density slightly 
heavier than that for a soft sugar and suddenly cooling the product, 
stirring all the time with a large spoon or paddle. This beating and 
cooling tends to produce microscopic crystals of sugar which give 
the product a creamy appearance and do not separate out on stand- 
ing if the proper density is maintained. An early run of sirup is 
not the best for this product, as some inversion of the sucrose is 
necessary to obtain the best results. This product has been called 
maple butter in some sections and is frequently prepared by farmers. 



42 BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 

Maple honey is the name often given to a light-colored maple 
sirup which has been boiled to a density slightly heavier than that 
of sap sirup, or similar to that of strained honey. The sirup could 
hardly be an early run, but should be one in which there has been 
some inversion of the sucrose, for otherwise the product will soon 
crystallize. As this substance has no connection with bees and is 
never stored in combs, the fitness of its name may be questioned. 

Maple wax is prepared by boiling sap sirup to a density nearly 
equal to that of hard sugar, but without stirring, and then pouring 
the product over snow or ice to secure an immediate cooling, thereby 
preventing crystallization of the sugar. This can be made only in 
small quantities and does not keep its waxy condition for any length 
of time. 

As in the case of maple sugar, chemical examination of these 
products should be carried on by concentrating them in solution to a 
sirup with a density of 65, calculating the analytical results so ob- 
tained to the moisture-free basis, and determining the original 
moisture content. 

CONCLUSIONS. 

ANALYTICAL FIGURES OF PURE MAPLE PRODUCTS. 

Moisture. — Maple sirup should have a density equivalent to at 
least 65 per cent dry substance or, in other words, it should weigh 
11 pounds to the gallon. A thinner product does not keep, and a 
heavier one shows more or less crystallization, depending on the 
quality of the sap and on manufacturing conditions. Maple sugar 
with a water content much over 5 per cent is runny and drains easily. 
In tub sugar, the moisture content may run as high as 10 to 12 per 
cent, but beyond this the sugar becomes mushy. 

Sugars. — Sucrose normally constitutes about 95 per cent of the 
dry substance of the maple product, and, together with about 3 per 
cent of reducing sugars, forms the total sugar content. In some 
samples sucrose constituted about 97.5 per cent of the product. In 
normal sirup, or sirup in which no acid fermentation has taken place, 
the sum of the sucrose and the reducing sugars calculated to sucrose 
by the factor 0.95 will give a figure ranging very close to 97.5 per 
cent of the dry substance. 

Ash. — The total ash is an important figure in the analysis of a 
maple product. The average percentage in 481 samples of maple 
sap sirup was found to be 1 per cent, with extremes of 1.68 and 0.68. 
In the 363 samples of maple sugars, the average was 0.98 per cent, 
with extremes of 1.70 and 0.76 per cent, all figured to a dry basis. 
Examining the results on these samples critically, we find that out of 
the 844 samples 10 have an ash content of 0.77 per cent or lower 
(Table XXIX). 



MAPLE SUGAR. 



43 



Table XXIX. — Samples of maple products with a total ash content of 0.77 per cent or 

less. 



Serial 
No. 


Total 
ash. 


Insoluble 
ash. 


Winton 

lead 
number. 


Malic 

acid 

value. 


Serial 
No. 


Total 

ash. 


Insoluble 
ash. 


Winton 

lead 
number. 


Malic 

acid 

value. 


6680 

8365 
8354 
8349 
8351 


Per cent. 
0.68 

.77 
.77 
.77 
.76 


Per cent. 
0.26 
.23 
.23 
.22 
.23 


2.22 
1.96 
2.13 
1.86 
1.85 


0.66 
.61 

1.15 
.92 

.78 


7743 
0) 
( x ) 

( 2 ) 
( 2 ) 


Per cent. 
0.76 

.77 
.77 
.76 
.77 


Per cent. 
0.45 
.22 
.22 
.25 
.24 


1.86 
2.04 
2.42 

1.87 
1.86 


0.75 
.62 
.61 
.62 
.60 



1 Taken from experimental work on change in color from sap to sugar sirup. 

2 Taken from experimental work on resugaring. 

Thus, in the examination of 844 samples, it is noted that a total 
ash content of 0.68 per cent has been found in one case only, and 
0.76 per cent in three cases only; all other samples give 0.77 per cent 
or over. In these four cases, all other figures are within those 
found in normal products, namely, Winton lead number 1.85 or 
over, insoluble ash 0.23 or over, and malic acid 0.59 or over. It 
seems then that percentages of ash lower than 0.77 per cent are 
abnormal figures and do not necessarily indicate a mixture with 
other sirup, especially cane-sugar sirups. 

The insoluble ash analysis is of equal importance with that of the 
total ash. Among the sap sirups the lowest insoluble ash content 
was found to be 0.23 per cent, with an average of 0.37 per cent and 
an extreme of 1.01 per cent. Three samples of sugar sirups had an 
insoluble ash content below 0.23 per cent, but the average was 0.36 
per cent and the extreme 1 per cent, practically the same as in the 
case of sap sirup. In the experimental work about five additional 
samples with an insoluble ash content of 0.22 per cent were found. 
The results on these eight samples appear in Table XXX. 

Table XXX. — Samples of maple products with an insoluble ash content below 0.23 per 

cent. 



Serial 
No. 


Total 
ash. 


Insoluble 
ash. 


Winton 

lead 
number. 


, Malic 

acid 

value. 


Serial 
No. 


Total 
ash. 


Insoluble 
ash. 


Winton 

lead 
number. 


Malic 

acid 

value. 


8349 

8344 
8330 
0) 


Per cent. 

0.77 

.78 

.81 

.77 


Per cent. 

0.22 

.21 

.22 

.22 


1.86 
1.85 
2.01 
2.04 


0.92 
.59 
.77 
.62 


( x ) 
0) 


Per cent. 

0.77 

.81 

.88 
.85 


Per cent. 

0.22 

.22 

.22 

.22 


2.42 
1.96 
2.20 
1.96 


0.61 

.60 
.66 
.69 



v i Taken from experimental work on change in color from sap to sugar sirup. 

All have a total ash content of 0.77 per cent or higher, a Winton 
lead number of 1.85 or higher, and a mafic acid value of 0.59 or 
higher. With the possible exception of No. 8344, these samples are 
abnormal in their insoluble ash content but normal in the other 
figures. Finding only 3 samples out of 844 with an insoluble ash 



44 



BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 



content lower than 0.23 per cent and with other figures normal, it 
seems fair to conclude that a pure maple product should have at 
least 0.23 per cent insoluble ash or, if it has less, that the other 
figures should be above the minima. 

Winton lead number. — Much stress is laid upon the Winton lead 
number in judging a maple product. Among the 481 sap sirups, the 
lowest number was 1.76, the next being 1.85, the highest 4.41, and 
the average 2.70. With the maple sugars, the lowest was 1.85, the 
highest 4.95, and the average 2.76. 



Table XXXI.- 


-Samples of maple products with a Winton lead number of 0.85 


or lower. 


Serial 
No. 


Total 
ash. 


Insoluble 
ash. 


Winton 

lead 
number. 


Malic 

acid 

value. 


Serial 
No. 


Total 
ash. 


Insoluble 
ash. 


Winton 

lead 
number. 


Malic 

acid 

value. 


6693 
6613 

6577 . . . 
6768... . 


Per cent. 
0.97 

.88 
.80 

.78 


Per cent. 

0.26 

.23 

.23 

.24 


1.76 
1.85 
1.85 
1.85 


0.31 
.79 
.73 
.80 


6635 

6827 
6891 
8344 


Per cent. 

0.91 

.77 

.83 
.78 


Per cent. 

0.27 

.23 

.35 

.21 


1.85 
1.85 
1.85 
1.85 


1.68 
.72 
.80 
.59 



The sample with 1.76 was abnormal in this respect, being the only 
one out of 844, but the other determinations are above the selected 
minima. The total ash in each case is 0.77 per cent or over, and 
in only one case, No. 8344, is the insoluble ash content below 0.23 
per cent. In two cases, however, the malic acid value is below 0.60. 
Here one sample only out of 844 has a lead number below 1.85, and 
as this sample is normal in ash and insoluble ash, 1.85 should be con- 
sidered the lower limit for such a figure. 

Ross lead number. — This determination was not made in the case 
of the sap sirups. It was made in 282 of the 283 sugar sirups from 
the United States and in 26 of the 80 sugar sirups from Canada. Of 
these 308 samples, only 6 cases were noted in which values of 2.35 or 
lower were obtained. The lowest value found was 2.20, the highest 
5.90, and the average 3.50. 

Table XXXII. — Samples of maple sugars with a Ross lead number of 2.35 or lower. 



Serial 


Total 


Insoluble 


Ross lead 


Malic acid 


Serial 


Total 


Insoluble 


Ross lead 


Malic acid 


No. 


ash. 


ash. 


number. 


value. 


No. 


ash. 


ash. 


number. 


value. 




Per cent. 


Per cent. 








Per cent. 


Per cent. 






8344 


0.78 


0.21 


2.20 


0.59 


7560 


0.78 


0.27 


2.31 


0.67 


6373 


.78 


.36 


2.22 


.74 


7512 


.78 


.23 


2.32 


.62 


6374 


.82 


.39 


2.25 


.83 


6617 


.78 


.34 


2.35 

» 


.62 



Of these six samples it is noted that, with the exception of 8344, 
determinations of other values do not fall below 0.77 total ash, 0.23 
insoluble ash, and 0.60 malic acid. As, with the exception of 8344, 
these samples are not found in Table XXXII, it is apparent that the 
Winton lead value also was not below 1.85. Even in the case of 



MAPLE SUGAR. 



45 



8344, the one apparently abnormal sample among some 844 samples, 
it is noted that all of the values do not fall below the minima just 
given. Applying the Ross lead number determination, which has 
been advanced for application in particular to mixtures of maple and 
cane sugar sirup, to pure maple products, it would appear that 2.25 
should be considered the lower limit for this value. 

Malic acid value. — Some food chemists lay great stress upon this 
determination, the minimum value for which in sap sirups was found 
to be 0.21, with an average of 1.01 and a maximum of 1.82. Only 
6 samples out of the 481 had a value below 0.60. In the sugar sirups, 
the lowest value was 0.51, the next lowest 0.59, and all the rest were 
above 0.60, the average being 0.93 and the extreme 1.72. Table 
XXXIII shows the analytical figures of the samples having a malic 
acid value lower than 0.60. 

Table XXXIII. — Samples of maple products with a malic acid value below 0.60. 



Serial 
No. 


Total 
ash. 


Insoluble 
ash. 


Winton 

lead 
number. 


Malic acid 
value. 


Serial 
No. 


Total 
ash. 


Insoluble 
ash. 


Winton 

lead 
number. 


Malic 
acid 
value. 


6693 
6692 
6773 
6918. 


Per cent. 
0.97 
1.01 

.77 
.89 


Per cent. 

0.26 

.24 

.26 

.26 


1.76 
2.36 
2.63 
1.86 


0.31 
.44 
.58 
.54 


6926 
6915 
8344 
8379 


Per cent. 
0.87 

.84 
.78 
.88 


Per cent. 

0.35 

.23 

.21 

.29 


1.98 
2.65 

1.85 
2.28 


0.52 
.21 
.59 
.51 



All these samples have a total ash content of 0.77 per cent or 
higher and with one exception an insoluble ash content of over 0.22. 
The lead number in each case, with one exception, is 1.85 or higher. 
It then seems proper to consider that a pure product must have a 
value of 0.60 per cent. Abnormal products may have a value below 
this, but they are not abnormal at the same time in ash or insoluble 
ash. 

Considering the subject as a whole, a pure maple product does not 
yield figures below the minima set. In one or two of the determina- 
tions it might give a figure below the minimum for such a determina- 
tion. If pure, however, it shows in the other determinations figures 
which exceed the minima. 

The minima set are: Total ash 0.77 per cent, calculated to dry 
basis; insoluble ash 0.23 per cent, calculated to dry basis; Winton 
lead number 1.85, calculated to dry basis; mafic acid value 0.60, 
calculated to dry basis. 

These apply also to the samples of maple sirups which Jones x re- 
ports as having lower minima. Of the 34 samples reported by him 
as being low in some particular, 6 show all figures below the minima 
just stated. The remainder are above in some of the determinations. 

i Vt. Agr. Exp. Sta. Bui. 167, p. 464. 



46 BULLETIN 466, U. S. DEPARTMENT OF AGRICULTURE. 

Table XXXIV. — Analytical figures of six samples showing low results. 1 

(Calculated to dry basis.] 



Sample No. 


Total ash. 


Insoluble 
ash. 


Malic acid 
value. 


Water in 
original 
sample. 


106 


Per cent. 
0.69 
.64 
.71 
.71 
.71 
.65 


Per cent. 
0.22 
.22 
.22 
.21 
.21 
.20 


0.59 
.59 
.56 
.58 
.44 
.49 


Per cent. 
30.48 


119 


28.75 


114 


30.69 


107 


27.90 


112 


31.34 


108 : 


29.64 







i Jones, Vt. Agr. Exp. Sta. Bui. 167, p. 464. 

The first three samples in Table XXXIV show an insoluble ash 
content only 0.01 per cent below the minimum set. Of these three, 
two have a malic acid value 0.01 per cent below the minimum; the 
other, one that is 0.03 below. This deviation is almost too slight to 
consider. Although low in malic acid values, the insoluble and 
total ash figures of the three remaining samples, with the exception 
of No. 108, approach very closely the minima set. A comparison 
with the data in Table V (page 6) indicates that, with the exception 
of the malic acid value, the analytical figures of sample 108 are 
increased if water is added and the concentration not carried too far. 



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